Electrochromic composition and electrochromic element
a technology of electrochromic elements and electrochromic compositions, applied in the field of electrochromic compositions, can solve the problems of reducing transparency, ct absorption in visible regions, easy reduction of cathodic ec compounds, etc., and achieves high colorless transparency in decoloration and suppresses ct interaction
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synthesis example 1
ary Compound B-4
[0173]
[0174]In a 50 mL reaction vessel, 300 mg (0.926 mmol) of XX-1 (5,5′-dibromo-2,2′-bithiophene) and 590 mg (3.24 mmol) of XX-2 were mixed with a toluene / 1,4-dioxane (6 ml / 6 ml) mixed solvent, and then dissolved oxygen was removed with nitrogen. Subsequently, 8.3 mg (0.037 mmol) of Pd(OAc)2 and 38 mg (0.093 mmol) of 2-dicyclohexyl phosphino-2′,6′-dimethoxy biphenyl (S-Phos), and 1.07 g (4.65 mmol) of tripotassium phosphate were added under a nitrogen atmosphere, heated and refluxed at 100° C., and then reacted for 6 hours. The reaction solution was cooled to room temperature, concentrated under reduced pressure, and then isolated and purified by silica gel chromatography (Mobile phase: Hexane / Chloroform=1 / 3), whereby B-4 of light yellow solid powder was obtained (240 mg).
[0175]As a result of confirming the structure of the compound B-4 by measurement of mass-spectrum (MS) measurement and nuclear magnetic resonance spectrum (NMR) measurement, the molecular weight a...
synthesis example 2
ary Compound A-14
[0177]
[0178](1) In a 100 mL reaction vessel, 2.0 g (10.8 mmol) of XX-3 was dissolved in 20 ml of THF. Subsequently, 1.93 g (10.8 mmol) of N-bromosuccinimide was added, and then stirred at room temperature for 2 hours. Water was added to the reaction solution, and then a precipitate was extracted with ethyl acetate and washed with water, whereby XX-4 was obtained (2.24 g).
[0179](2) In a 50 ml reaction vessel, 1.0 g (3.8 mmol) of XX-4 was dissolved in 9 ml of DMF. 0.167 g (4.18 mmol) of sodium hydride (60%) was added to the solution under a nitrogen stream, and then stirred at room temperature for 1 hour. To the solution, 0.54 ml (4.56 mmol) of benzyl bromide was added dropwise, and then stirred at room temperature for 3 hours. The reaction solution was concentrated under reduced pressure, and then isolated and purified by silica gel chromatography (Mobile phase: Hexane / Ethyl acetate=5 / 1), whereby XX-5 was obtained (0.99 g).
[0180](3) In a 50 mL reaction vessel, 0.99 g...
example 2
[0189]A mixed solution was produced in the same manner as in Example 1, except using Exemplary Compound C-5 as a cathodic EC compound, and then the wavelength shift amount was calculated from an absorption spectrum thereof. The result was shown in Table 1.
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